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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Optimizing Batch Crystallization with Model-based Design of Experiments

Poster for Foundations of Computer Aided Process Design (FOCAPD) 2024 describing the formality of model-based design of experiments for batch crystallization. This paper focuses on the implementation of model-based design of experiments for parameter precision, enabled by Pyomo.DoE, a package in Python. Specifically, this work outlines an identifiability analysis for the estimability of the model parameters in a batch crystallization system.

Lynch, Hailey↗
DOE OSTI2016

Impact of scaling on the nitric-glycolic acid flowsheet

Savannah River Remediation (SRR) is considering using glycolic acid as a replacement for formic acid in Sludge Receipt and Adjustment Tank (SRAT) processing in the Defense Waste Processing Facility (DWPF). Catalytic decomposition of formic acid is responsible for the generation of hydrogen, a potentially flammable gas, during processing. To prevent the formation of a flammable mixture in the offgas, an air purge is used to dilute the hydrogen concentration below the 60% of the Composite Lower Flammability Limit (CLFL). The offgas is continuously monitored for hydrogen using Gas Chromatographs (GCs). Since formic acid is much more volatile and toxic than glycolic acid, a formic acid spill would lead to the release of much larger quantities to the environment. Switching from formic acid to glycolic acid is expected to eliminate the hydrogen flammability hazard leading to lower air purges, thus downgrading of Safety Significant GCs to Process Support GCs, and minimizing the consequence of a glycolic acid tank leak in DWPF. Overall this leads to a reduction in process operation costs and an increase in safety margin. Experiments were completed at three different scales to demonstrate that the nitric-glycolic acid flowsheet scales from the 4-L lab scale to the 22-L bench scale and 220-L engineering scale. Ten process demonstrations of the sludge-only flowsheet for SRAT and Slurry Mix Evaporator (SME) cycles were performed using Sludge Batch 8 (SB8)-Tank 40 simulant. No Actinide Removal Process (ARP) product or strip effluent was added during the runs. Six experiments were completed at the 4-L scale, two experiments were completed at the 22-L scale, and two experiments were completed at the 220-L scale. Experiments completed at the 4-L scale (100 and 110% acid stoichiometry) were repeated at the 22-L and 220-L scale for scale comparisons.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2017

Chromatographic separation of radioactive noble gases from xenon

The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes 85 Kr and 39 Ar that are not removed by the in situ gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search exmperiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400 kg of xenon was processed, reducing the average concentration of krypton from 130 ppb to 3.5 ppt as measured by a cold-trap assisted mass spectroscopy system. Finally, a 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2025

Custom Equipment Development for Processing of Surplus Plutonium

The Strategic Laboratory Assessment (SLA), a collaborative team of SRNL and ORNL personnel, has been established to advance the objectives of the Surplus Plutonium Disposition (SPD) Project, by identifying and developing technologies to accelerate disposition, reduce life cycle costs, minimize worker radiation exposure, improve worker safety, and minimize Surplus Plutonium Disposition Program risks. [1] The SLA team has identified can cutting and plutonium (Pu) oxide size reduction as two glovebox processes where technology enhancements would be valuable. The DOESTD-3013 package currently in use for Pu downblending requires cutting two nested cans before the inner convenience can that holds the Pu oxide may be accessed for further processing. A rotary tubing-style cutter is used for opening the 3013 packages within the glovebox. Collet changeouts are required between cutting of the outer and inner cans. The SLA team is currently developing and testing an adjustable-clamp can cutter design that eliminates collet changeouts and allows cutting of the outer and inner can at the same time, resulting in significant reduction of radiological dose and process time, as well as improved ergonomics. To meet the Pu oxide particle size requirement, size reduction of Pu oxide agglomerations must be performed within the process gloveboxes. The SLA team has identified jaw crushing technology as an alternative to the currently employed rotary mill. Jaw crusher advantages include reduced dust within the glovebox, increased batch sizes, and easier integration with other glovebox processes due to the flow-through nature of jaw crushing. Commercially manufactured jaw crushers are either too large and/or too heavy for implementation in the SPD gloveboxes, so the SLA team is developing and testing a custom jaw crusher to meet the needs of the SPD Project.

Krementz, Daniel [Savannah River National Laborato↗
DOE OSTI2022

No ball milling needed: Alternative ODS steel manufacturing with gas atomization reaction synthesis (GARS) and friction-based processing

Oxide dispersion strengthened (ODS) steels are promising structural materials for future fusion reactors. The high-density (~10 23 /m 3 ) of highly stable Y-(Ti)-O nano-oxides provide high sink strength for radiation resistance and high-temperature (> 650 °C) creep strength. Concomitantly, helium management is enabled by trapping high density (~10 23 /m 3 ) of small (< 3 nm) helium bubbles in the vicinity of nano-oxides. However, conventional route of making ODS steels involves prolonged ball milling, canning, degassing, and laborious thermo-mechanical processing (TMP). Such route, especially the batch-by-batch ball milling step, faces persistent challenge with scalability and high costs. Gas atomization reaction synthesis (GARS) method has demonstrated the potential of making precursor ODS steel powders without ball milling, but the nano-oxide density was around 10 21 /m 3 in the final consolidated form by conventional TMP. Taking advantage of GARS precursor powder, we use friction-based processing, including friction consolidation and extrusion, to manufacture ODS steel with further improved nano-oxide characteristics. Here, preliminary results showed that Y/Ti/O species were intimately mixed and rapidly reacted to form nano-oxides with a number density of ~10 22 /m 3 .

36 MATERIALS SCIENCE↗
DOE OSTI2016

DWPF Melter Off-Gas Flammability Assessment for Sludge Batch 9

The slurry feed to the Defense Waste Processing Facility (DWPF) melter contains several organic carbon species that decompose in the cold cap and produce flammable gases that could accumulate in the off-gas system and create potential flammability hazard. To mitigate such a hazard, DWPF has implemented a strategy to impose the Technical Safety Requirement (TSR) limits on all key operating variables affecting off-gas flammability and operate the melter within those limits using both hardwired/software interlocks and administrative controls. The operating variables that are currently being controlled include; (1) total organic carbon (TOC), (2) air purges for combustion and dilution, (3) melter vapor space temperature, and (4) feed rate. The safety basis limits for these operating variables are determined using two computer models, 4-stage cold cap and Melter Off-Gas (MOG) dynamics models, under the baseline upset scenario - a surge in off-gas flow due to the inherent cold cap instabilities in the slurry-fed melter.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Dispersion-enhanced sequential batch sampling for adaptive contour estimation

In computer simulation and optimal design, sequential batch sampling offers an appealing way to iteratively stipulate optimal sampling points based upon existing selections and efficiently construct surrogate modeling. Nonetheless, the issue of near duplicates poses tremendous quandary for sequential learning. It refers to the situation that selected critical points cluster together in each sampling batch, which are individually but not collectively informative towards the optimal design. Near duplicates severely diminish the computational efficiency as they barely contribute extra information towards update of the surrogate. To address this issue, we impose a dispersion criterion on concurrent selection of sampling points, which essentially forces a sparse distribution of critical points in each batch, and demonstrate the effectiveness of this approach in adaptive contour estimation. Specifically, we adopt Gaussian process surrogate to emulate the simulator, acquire variance reduction of the critical region from new sampling points as a dispersion criterion, and combine it with the modified expected improvement (EI) function for critical batch selection. The critical region here is the proximity of the contour of interest. This proposed approach is vindicated in numerical examples of a two-dimensional four-branch function, a four-dimensional function with a disjoint contour of interest and a time-delay dynamic system.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2019

Enhanced Light Extraction from Low Cost White OLEDs Fabricated on Novel Patterned Substrates” (Final Report)

Organic LEDs (OLEDs) are a very attractive emerging solid state lighting (SSL) technology. Currently, one of the main challenges is to increase the extraction of the light generated inside the OLED into the forward (viewing) hemisphere. In conventional OLEDs fabricated on a transparent flat anode coated on glass the outcoupling factor is only about 20%. About 50% of the light is lost at the metal cathode (surface plasmon excitation), and waveguided internally in the organic layers and the transparent anode. Another ~30% is waveguided in the substrate to its edges. The research addressed this issue of outcoupling by evaluating OLEDs fabricated on corrugated plastic substrates manufactured in a cost-effective approach. It demonstrated that the outcoupling from such OLEDs can exceed 50% by mitigating plasmon–related loss and internal waveguiding, even without the addition of a microlens array or a hemispherical lens, either of which extracts the light trapped in the substrate. Simulations conducted in parallel with the experimental effort demonstrated how the corrugation assists in the outcoupling. The project also evaluated the role of the corrugation pitch and height in determining the outcoupling factor and other properties of the OLEDs. The technical effectiveness and economic feasibility of the project lie in the patterning of the extracting plastic substrates in an approach that is scalable to roll-to-roll (R2R) manufacturing. R2R processes are drastically lower-cost than batch or single-unit fabrication. The corrugated plastic substrates studied are part of an integrated substrate that includes also a microlens array at the air-side of the substrate and a conductive electrode. The project that was a university-industry collaboration is of major benefit to the public as it demonstrates the feasibility of manufacturing highly efficient OLEDs for SSL in a R2R process, which would drastically reduce the manufacturing cost and increase production in the USA. SSL is efficient and environmentally-friendly. It reduces electricity consumption, and hence lighting cost.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2025

Creating a Salt Batch: Challenges and Lessons Learned

CONCLUSION • The overall Salt Batch system has been honed through each iteration of the process • Increased communication across facilities and work groups has enabled the salt team to react swiftly to emergent items and identify improvement opportunities • Even the best plans require backup options – Emergent items can appear at any time during the process – Flexibility to adapt to the unexpected is a must-have team mindset • To date, every salt batch compiled has been qualified and approved as feed for SWPF – No feed break has occurred between the Tank Farm and SWPF

Goldblatt, Joshua B. [Savannah River National Labo↗
NASA NTRS1998

Effects of Fiber Coating Composition on Mechanical Behavior of Silicon Carbide Fiber-Reinforced Celsian Composites

Celsian matrix composites reinforced with Hi-Nicalon fibers, precoated with a dual layer of BN/SiC by chemical vapor deposition in two separate batches, were fabricated. Mechanical properties of the composites were measured in three-point flexure. Despite supposedly identical processing, the composite panels fabricated with fibers coated in two batches exhibited substantially different mechanical behavior. The first matrix cracking stresses (sigma(sub mc)) of the composites reinforced with fibers coated in batch 1 and batch 2 were 436 and 122 MPa, respectively. This large difference in sigma(sub mc) was attributed to differences in fiber sliding stresses(tau(sub friction)), 121.2+/-48.7 and 10.4+/-3.1 MPa, respectively, for the two composites as determined by the fiber push-in method. Such a large difference in values of tau(sub friction) for the two composites was found to be due to the difference in the compositions of the interface coatings. Scanning Auger microprobe analysis revealed the presence of carbon layers between the fiber and BN, and also between the BN and SiC coatings in the composite showing lower tau(sub friction). This resulted in lower sigma(sub mc) in agreement with the ACK theory. The ultimate strengths of the two composites, 904 and 759 MPa, depended mainly on the fiber volume fraction and were not significantly effected by tau(sub friction) values, as expected. The poor reproducibility of the fiber coating composition between the two batches was judged to be the primary source of the large differences in performance of the two composites.

Bansal, Narottam P.↗
DOE OSTI2020

Data optimization for large batch distributed training of deep neural networks

Distributed training in deep learning (DL) is common practice as data and models grow. The current practice for distributed training of deep neural networks faces the challenges of communication bottlenecks when operating at scale, and model accuracy deterioration with an increase in global batch size. Present solutions focus on improving message exchange efficiency as well as implementing techniques to tweak batch sizes and models in the training process. The loss of training accuracy typically happens because the loss function gets trapped in a local minima. We observe that the loss landscape minimization is shaped by both the model and training data and propose a data optimization approach that utilizes machine learning to implicitly smooth out the loss landscape resulting in fewer local minima. Our approach filters out data points which are less important to feature learning, enabling us to speed up the training of models on larger batch sizes to improved accuracy.

Gahlot, Shubhankar↗
DOE OSTI2014

DEVELOPMENT OF AN ANTIFOAM TRACKING SYSTEM AS AN OPTION TO SUPPORT THE MELTER OFF-GAS FLAMMABILITY CONTROL STRATEGY AT THE DWPF

The Savannah River National Laboratory (SRNL) has been working with the Savannah River Remediation (SRR) Defense Waste Processing Facility (DWPF) in the development and implementation of an additional strategy for confidently satisfying the flammability controls for DWPF’s melter operation. An initial strategy for implementing the operational constraints associated with flammability control in DWPF was based upon an analytically determined carbon concentration from antifoam. Due to the conservative error structure associated with the analytical approach, its implementation has significantly reduced the operating window for processing and has led to recurrent Slurry Mix Evaporator (SME) and Melter Feed Tank (MFT) remediation. To address the adverse operating impact of the current implementation strategy, SRR issued a Technical Task Request (TTR) to SRNL requesting the development and documentation of an alternate strategy for evaluating the carbon contribution from antifoam. The proposed strategy presented in this report was developed under the guidance of a Task Technical and Quality Assurance Plan (TTQAP) and involves calculating the carbon concentration from antifoam based upon the actual mass of antifoam added to the process assuming 100% retention. The mass of antifoam in the Additive Mix Feed Tank (AMFT), in the Sludge Receipt and Adjustment Tank (SRAT), and in the SME is tracked by mass balance as part of this strategy. As these quantities are monitored, the random and bias uncertainties affecting their values are also maintained and accounted for. This report documents: 1) the development of an alternate implementation strategy and associated equations describing the carbon concentration from antifoam in each SME batch derived from the actual amount of antifoam introduced into the AMFT, SRAT, and SME during the processing of the batch. 2) the equations and error structure for incorporating the proposed strategy into melter off-gas flammability assessments. Sample calculations of the system are also included in this report. Please note that the system developed and documented in this report is intended as an alternative to the current, analytically-driven system being utilized by DWPF; the proposed system is not intended to eliminate the current system. Also note that the system developed in this report to track antifoam mass in the AMFT, SRAT, and SME will be applicable beyond just Sludge Batch 8. While the model used to determine acceptability of the SME product with respect to melter off-gas flammability controls must be reassessed for each change in sludge batch, the antifoam mass tracking methodology is independent of sludge batch composition and as such will be transferable to future sludge batches.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Deployment of Low Temperature Aluminum Dissolution (LTAD) Technology to Retrieve H-Modified (HM) Sludge in SRS Tank 15 – 25672

Tank 15 is a 4,234,000-liter (1,118,500-gallon) Type 2 high-level waste storage tank located in H Tank Farm at the Savannah River Site. It was put into service in 1960 to receive high-activity, H-Modified (HM) waste from H Canyon. Between June 1964 and November 1972, the waste tank was filled six times, and supernate was decanted five times, leaving behind the sludge solids. Tank 15 also received a mixture of high-activity and low-activity HM waste from Tank 16. Tank 15 has more recently undergone several mixing campaigns to remove much of the sludge waste; however, the effectiveness of suspending the sludge heel via mechanical mixing has significantly diminished. Low Temperature Aluminum Dissolution (LTAD) is a process developed for the dissolution of suspended aluminum solids in a large waste storage tank. Originally intended for deployment during the preparation of sludge batches in H Tank Farm for the Defense Waste Processing Facility (DWPF), the process involves maintaining the waste storage tank at a slightly elevated temperature and highly alkaline chemistry to facilitate dissolution of aluminum solids. As mechanical heel removal efforts diminished in effectiveness in Tank 15, LTAD was selected to both reduce the volume of sludge solids remaining in the heel and to modify the sludge rheology to facilitate the suspension of additional solids using the installed mixing devices.

Campbell, Seth G.↗
DOE OSTI2026

How exudates production along a phosphorus gradient influences mineral dissolution across contrasting soil development stages

Harnessing rhizosphere processes offers a valuable opportunity to optimize nutrient use efficiency in agroecosystems. In nutrient-limited soils, plants discharge part of photosynthate surplus via root exudation, including carboxylates, which may enhance mineral dissolution and nutrient mobilization. We aimed to assess how plant responses to nutrient limitation translated into changes in exudate profiles, and how these exudates, in turn, drive bioweathering processes across soils of contrasting mineralogy and weathering degree. We conducted a hydroponic experiment with Lupinus albus grown under five phosphorus (P) concentrations (5, 10, 20, 30, and 50 µM) over seven weeks. We measured plant biomass and root traits, performed a metabolomics analysis and quantified seven carboxylates in root exudates using gas chromatography-mass spectrometry. To assess bioweathering processes across contrasted soil domains, we conducted batch dissolution tests with exudates using three soil horizons—35 each with distinct physicochemical properties: enriched in organic matter, iron oxides, or primary silicates. At the intermediate level of P supply, shoot biomass was comparable to that under high P, but plants produced more root biomass and a higher total carboxylate exudation rate. Despite low carboxylate concentrations (<100 ppb), exudates promoted the dissolution of Ca, Mg, Si, Fe, P and K in all horizons. Yet, the degree of element released varied among horizons. These findings highlight the importance of root exudates in enhancing mineral dissolution, with effects dependent on soil physicochemical properties. The results suggest that managing agroecosystems under moderate nutrient limitation could be a sustainable strategy to increase root-to-shoot ratios, enhance bioweathering processes and nutrient release in soil solution.

Pollet, Sasha L.↗
NASA NTRS1980

A description of a system of programs for mathematically processing on unified series (YeS) computers photographic images of the Earth taken from spacecraft

A description of a batch of programs for the YeS-1040 computer combined into an automated system for processing photo (and video) images of the Earth's surface, taken from spacecraft, is presented. Individual programs with the detailed discussion of the algorithmic and programmatic facilities needed by the user are presented. The basic principles for assembling the system, and the control programs are included. The exchange format within whose framework the cataloging of any programs recommended for the system of processing will be activated in the future is displayed.

Zolotukhin, V. G.↗
DOE OSTI2020

Development of Spouting Bed Reactor for Reduction of Hematite to Magnetite (Final Report)

This project was designed to leverage both past and current technology development efforts and utilize the expertise of the National Energy Technology Laboratory (NETL) in a collaborative effort with SIOX for the development of a spouting bed reactor to produce magnetite from very fine hematite waste. More specifically, the effort involved the conversion of a steel manufacturing byproduct, iron oxide hematite (Fe 2 O 3 ), and reduces it chemically into a salable magnetite product applicable to a number of markets. SIOX previously operated a magnetite batch production facility based on a rotary kiln reactor process. Unfortunately, that process was both costly and inefficient, making it difficult to achieve desired economies, purity, and throughput levels. NETL’s technology, developed in this work, replaced the batch inefficient rotary kiln with a continuous spouting bed reactor capable of producing synthetic magnetite products. In the project, NETL was to develop the spouting bed for the SIOX application and SIOX was to construct and operate a fully integrated pilot scale demonstration plant. NETL successfully completed its tasks, but SIOX due to financial issues was not able to complete their tasks. They have chosen not to participate in this final report so for their tasks a short summary of NETL’s knowledge of their efforts is included.

36 MATERIALS SCIENCE↗
NASA NTRS2009

A Study on Advanced Lithium-Based Battery Cell Chemistries to Enhance Lunar Exploration Missions

NASA's Exploration Technology Development Program (ETDP) Energy Storage Project conducted an advanced lithium-based battery chemistry feasibility study to determine the best advanced chemistry to develop for the Altair lunar lander and the Extravehicular Activities (EVA) advanced lunar surface spacesuit. These customers require safe, reliable energy storage systems with extremely high specific energy as compared to today's state-of-the-art batteries. Based on customer requirements, the specific energy goals for the development project are 220 watt-hours per kilogram (Wh/kg) delivered at the battery level at 0 degrees Celsius (degrees Celcius) at a C/10 discharge rate. Continuous discharge rates between C/5 and C/2, operation over 0 to 30 degrees C, and 200 cycles are targeted. The team, consisting of members from NASA Glenn Research Center, Johnson Space Center, and Jet Propulsion laboratory, surveyed the literature, compiled information on recent materials developments, and consulted with other battery experts in the community to identify advanced battery materials that might be capable of achieving the desired results with further development. A variety of electrode materials were considered, including layered metal oxides, spinel oxides, and olivine-type cathode materials, and lithium metal, lithium alloy, and silicon-based composite anode materials. lithium-sulfur systems were also considered. Hypothetical cell constructs that combined compatible anode and cathode materials with suitable electrolytes, separators, current collectors, headers, and cell enclosures were modeled. While some of these advanced materials are projected to obtain the desired electrical performance, there are risks that also factored into the decision making process. The risks include uncertainties due to issues such as safety of a system containing some of these materials, ease of scaling-up of large batches of raw materials, adaptability of the materials to processing using established or reasonable cost manufacturing techniques, manufacturability of the materials in dimensions required for integration into battery cells of practical capacities, low Technology Readiness levels (TRl), and the ability to achieve the desired performance by the customer need dates. The advanced cell chemistry options were evaluated with respect to multiple quantitative and qualitative attributes while considering their projected performance at the end of the available development timeframe. Following a rigorous ranking process, a chemistry that combines a lithiated nickel manganese cobalt oxide (lithium NMC) cathode with a silicon-based composite anode was selected as the technology that can offer the best combination of safety, specific energy, energy density, and likelihood of success. Tasks over the next three years will focus on development of electrode materials, compatible electrolytes, and separator materials, and integration of promising components to assess their combined performance in working cells. Cells of the chosen chemistry will be developed to TRl 6 by 2014 and will then be transferred to the customers for infusion into their mission paths.

Reid, Concha↗
DOE OSTI2022

Solvent Recovery and Management at the Savannah River Site H-Canyon Facility

NIOWAVE, Inc. is a domestic supplier of medical and industrial isotopes from uranium and radium. The Savannah River National laboratory (SRNL) is currently providing support to NIOWAVE, which plans to deploy a superconducting electron linear accelerator (LINAC) to fission uranium for Mo-99 production without the need for a nuclear reactor or HEU. The uranium from the Mo-99 production targets will be purified using a modified PUREX (Plutonium Uranium Reduction Extraction) solvent extraction process to recover the uranium in the product stream. The uranium will then be precipitated as an oxalate which is calcined to U 3 O 8 to fabricate pellets for new Mo-99 targets. In previous support provided to NIOWAVE, the SRNL demonstrated a solvent washing process to remove degradation products from the tributyl phosphate (TBP) solvent used in the modified PUREX process under development for uranium recovery. To supplement this technology demonstration, NIOWAVE requested the SRNL to provide summary information on the solvent recovery and management activities which are used at the Savannah River Site (SRS) H-Canyon facility. An existing reference document for the reprocessing of irradiated HEU fuels at the SRS was used as the primary reference for the solvent management activities; although, other reference documents were used to provide supplementary information. The information provided includes a brief summary of the solvent degradation issues which have been observed in the H-Canyon solvent extraction cycles and resulting process safety concerns. The solvent recovery processes for the three cycles of solvent extraction used in the H-Canyon were subsequently described including the process equipment which consists of the continuous and batch solvent washers, pumps, and tanks. A final section is provided on the monitoring and analysis of solvent quality based on the previous work performed at the SRNL for NIOWAVE and past research and development activities performed to support the solvent extraction processes in both the SRS F-Canyon and H-Canyon facilities.

07 ISOTOPE AND RADIATION SOURCES↗